Method for catalytic synthesis of tributyl citrate by utilizing immobilized p-toluenesulfonic acid

A technology of tributyl citrate and p-toluenesulfonic acid is applied in the chemical industry, and can solve the problems of complex post-treatment process, many catalyst side reactions, complex preparation process and the like, achieve easy recovery and reuse, and improve the efficiency of esterification reaction. , The effect of simplifying the post-processing process

Active Publication Date: 2012-07-04
BENGBU BBCA MEDICINE SCI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional production process uses concentrated sulfuric acid as a catalyst, but this catalyst has many side reactions, difficult refining, serious equipment corrosion, complicated post-treatment process, and waste acid pollution. Its application has

Method used

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  • Method for catalytic synthesis of tributyl citrate by utilizing immobilized p-toluenesulfonic acid
  • Method for catalytic synthesis of tributyl citrate by utilizing immobilized p-toluenesulfonic acid
  • Method for catalytic synthesis of tributyl citrate by utilizing immobilized p-toluenesulfonic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1) Preparation of immobilized p-toluenesulfonic acid

[0023] Take 2.5g of sodium alginate, 5g of polyvinyl alcohol and 1.5g of p-toluenesulfonic acid, add it to 100mL of deionized water, mix well, heat it in a constant temperature water bath at 80°C to completely dissolve it, and cool it to about 45°C with a constant temperature The flow pump drops it into 100 mL of calcium chloride solution with a mass percentage of 1.5% at a speed of 60 rpm and continuously stirs it slowly. Then take out and filter to obtain immobilized p-toluenesulfonic acid.

[0024] 2) Esterification reaction

[0025] Add 308g n-butanol, 200g citric acid, immobilized p-toluenesulfonic acid prepared in step 1) into a 500mL three-necked flask equipped with electromagnetic stirring, thermometer, reflux condenser, and water separator, heat under reflux at 130°C and stir, The water produced by the reaction is separated from the water separator, and the reaction is stopped when it is no water and then...

Embodiment 2-4

[0029] Only change the amount of n-butanol, and the rest are the same as in Example 1. The results are shown in Table 1.

[0030] Table 1

[0031]

Embodiment 5-7

[0033] Only the esterification temperature was changed, and the rest were the same as in Example 1. The results are shown in Table 2.

[0034] Table 2

[0035]

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Abstract

The invention provides a method for catalytic synthesis of tributyl citrate by utilizing immobilized p-toluenesulfonic acid, comprising the steps of taking the immobilized p-toluenesulfonic acid as a catalyst, carrying out esterification reaction on citric acid and n-butyl alcohol and synthetizing the tributyl citrate. The method provided by the invention has the advantages that: the immobilized p-toluenesulfonic acid adopted as the catalyst has no obvious corrosivity and is easy to recover and repeatedly utilize, the activity of the recovered catalyst basically remains unchanged; the esterification reaction efficiency is increased and the product yield can be up to 97.2-99.6%; adopting the reactant n-butyl alcohol as a water-carrying agent not only avoids the use of toxic solvents such as toluene and the like but also simplifies the aftertreatment process; the esterification reaction is mild in condition and simple in process, and the method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of chemical industry, in particular to a method for catalyzing and synthesizing tributyl citrate with immobilized p-toluenesulfonic acid. Background technique [0002] Tributyl citrate is a new type of non-toxic plasticizer. It has the characteristics of good compatibility, high plasticizing efficiency, non-toxicity, low volatility, cold resistance, mildew resistance, light resistance and water resistance. At present, the commonly used plasticizers in the industry are phthalates. Because they can induce cancer, their use has been strictly controlled in foreign countries. my country has also formulated relevant regulations to gradually eliminate their use in food packaging materials, medical appliances, and toys. use, and use tributyl citrate as a new substitute, so it has excellent development and application prospects. [0003] Tributyl citrate is usually esterified by citric acid and n-butanol under the action of a ...

Claims

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Application Information

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IPC IPC(8): C07C69/704C07C67/08
Inventor 陶涛汪洪湖张亚孙建华韦亚锋李亚龙
Owner BENGBU BBCA MEDICINE SCI DEV
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